Waters introduced the Alliance iS High Performance Liquid Chromatography System at Booth #1648.
Pittcon 2023 attracted about 8,000 conferees and vendors to the Pennsylvania Convention Center in Philadelphia March 18 to 22, 2023. The COVID-19 pandemic interrupted the last three meetings, so vendors and conferees had a lot to catch up on. Three years of advances in applications, technology and services were crammed into three days. Everyone was busy, and pleasant surprises were frequent and significant. On a personal note, I’ve been to over 50 Pittcon meetings and 2023 was the best!
This year’s report will focus on new technology and enabled applications, as well as a few new instruments in the separations and chromatographic arenas.
Environmental
Applications attracting the most interest were environmental, in particular PFAS, power, artificial intelligence (AI) and workflow automation.
For example, Syft Technologies introduced their next-gen SIFT-MS called the Syft Tracer. The Tracer provides a major performance upgrade in speed and detection limits. SIFT stands for Selected Ion Flow Tube, where soft chemical ionization provides real-time assays of volatile organic analytes in gases, including air with lower ppt detection limits. This obviates the need for concentration and chromatography.
Post-column derivatization is often the detection technology of choice for several applications, including paralytic shellfish toxins, mycotoxins, carbamate pesticides, glyphosate herbicides, and bromate. During the last 35 years, Pickering Laboratories has developed a series of post-column reactor modules, first for amino acids, but rapidly spreading to other needs where excellent detection sensitivity and specificity are important. This year, Pickering introduced the Onyx PCX, which includes a column oven controlling within 1 oC of set point for improved reaction control and assay precision. Quick-Change reactor cartridges reduce down-time. The Onyx also uses pulseless syringe pumps to deliver the reagents.
Deanna Bissonnette, an applications chemist at Biotage, discussed improvements in EPA Method 608.3 for pesticide assay of wastewater and Method 508 (Pesticides in drinking water with Solid Phase Extraction (SPE)). Her improvements involved reducing the sample volume from one liter to 100 mL. The SPE extract is less than 15 mL, which requires only 15 minutes for solvent blow down and exchange.
Doo Soo Chung, professor of chemistry at Seoul National University, reported a method for pesticide analysis of fruit by high-performance capillary electrophoresis (HPCE). His method, called Liquid Extraction Surface Analysis (LESA), directly samples analytes on a surface, thus avoiding unnecessary dilution by homogenization of the bulk sample. This is possible when non-infiltrative pesticides remain on the fruit skin. A commercial HPCE equipped with two capacitance detectors facilitated detection of anionic and cationic pesticides in a single run. Chung also used LESA to study anode material lithium batteries.
As we move to a circular economy, many materials, including plastics, will be included in post-consumer recycling. This may entail more rigorous quality control than the original product. Nadin Boegelsack at SepSolve Analytical spoke on methods for malodors in post-consumer recycling of plastics. Aliphatic hydrocarbons can be detected by 1D GC-MS. But these are not as potent stinkers as the oxygenated degradants. Solid phase micro extraction (SPME) and headspace methods lack sufficient detection sensitivity. Boegelsack found that thermal desorption coupled with 2D GC (TD-GCXGC-TOF MS) is much more effective in detecting and identifying malodorous analytes in a complex matrix such as weathered plastics. For more routine QC, the TOF-MS can be replaced by a flame ionization detector (FID).
Power, energy and batteries
At a press conference, JEOL described how their instruments are used to study the structural details of lithium-ion batteries. The Japanese-based manufacturer has developed an air-isolated workflow to study lithium metal in batteries in research and production. JEOL’s NMRs are also used to study the microenvironment and migration of lithium ions in lithium-ion batteries.
Magritek introduced their Spinsolve 90, which is a desktop NMR spectrometer capable of characterizing the environment of 1H, 13C, 7Li, 11B, 15N, 19F, 23Na, 29Si, and 31P nuclei. The Halbach permanent magnet obviates the need for cryogens. Individual samples are introduced in NMR tubes or flow-through, for on-line reaction monitoring. Booth staff reported that battery research focused on lithium was a new hot topic.
Recent interest in improving battery efficiency and durability is paying off. However, parasitic side reactions, which lower efficiency of lithium-ion batteries, are difficult to evaluate. TA Instruments introduced a TAM IV Microcalorimeter coupled to a Biologics VSP-300 Potentiostat to enable measurement of heat flow in batteries. This correlates with electrochemical events such as repetitive charge/discharge cycles. The system facilitates determination of power lost due to non-reversible side reactions, which lowers efficiency and lifetime. The cycler can process 12 battery samples in parallel.
Battery anodes are also a hot topic in modern battery development. Micromeritics introduced their TriStar ll plus instrument targeted on improving the energy density of anodes including graphite, graphene and graphene oxide. The Tristar measures the nitrogen isotherm from which scientists can extract the surface area and pore size distribution. As an illustrative example, graphene oxide showed an heterogenous surface of basal and prismatic planes, defects and micro pores at 100 oK.
Artificial intelligence
With all the hype surrounding AI, one wonders what AI might mean for the lab. JEOL provided an example with GC-HR-TOF-MS with training sets for drugs of abuse and another for cannabis. Suppose one sees a mystery peak in one run — what could it be? There might be 100,000 possible structures. First, the peak is analyzed by electron impact ionization, which gives the isotopic abundances that are mapped to the elemental composition (C, H, O, N, …hetero). Next, the MS uses one of the soft ionization sources such as chemical ionization (CI) to record the fragmentation pathways. The data is fed to JEOL’s msFineAnalysis AI software. The software is very fast, providing a list of candidates including knowns plus predicted structures, never seen before, in about three minutes. The program runs exclusively on JEOL’s AccuTOF GC-alpha.
JEOL’s GC-HR-TOF-MS is their sixth generation of GC-MS. It boasts resolving power greater than 30,000 with mass inaccuracy of less than 1 ppm. JEOL expects that the system will be particularly useful in analysis of natural and synthetic fuels and oils.
Liquid chromatography
At the Chromatography Forum of the Delaware Valley session, Robert Kennedy, professor at the University of Michigan, gave a lecture on pushing the limits of liquid chromatography for speed and efficiency. Some figures of merit he mentioned, included:
- Separation time: 10 to 15 seconds with novel detector.
- Pressure limit of mobile phase: 40,000 psi.
- Diameter of column packing: 1.1 μm.
- Column length: 20 to 50 cm.
The benefit is high speed and throughput. Plus, improved lower detection limit since the peaks are very narrow. The high efficiency enables higher peak count of complex samples.
Waters introduced the Alliance iS High Performance Liquid Chromatography System designed to reduce lab errors by 40%, especially in high-volume QC laboratories. Last year, Waters surveyed more than 50 laboratories that had more than 25 QC HPLCs. From this, they developed a model that supports the predicted impact (~40% error rate) of behind-the-panel-smarts.
The reduction will certainly increase productivity and data reliability. The iS is controlled by Waters Empower system software. Plus, the iS line of columns enables computerized tracking of the history and performance of individual columns with the eConnect RFI implemented sub system. Other design features include: quaternary gradient elution; tunable dual wavelength UV detector; Pmax: 10,000 psi; stainless steel sample flow path; and sample capacity of plates with 24 to 384 wells.
When starting a new day or sample queue, the large touch screen presents the key performance indicators, including oven temperature, column identification with injection counts, and mobile phase program. This can be compared with the set points in the prescribed method. Other checkpoints for system qualification include: missing sample vial, insufficient mobile phase in any reservoir, and need for scheduled maintenance. The iS also communicates with enterprise data systems so laboratory managers can view the status of any of their fleet of HPLCs.
The Bruker brand spans a wide range of mass spectrometers, but for LC-MS, this is only half the package. Bruker developed the Compass Hystar software for LC-MS with a range of commercial HPLCs. However, many chemists preferred single vendor responsibility. Bruker responded with introduction of the nanoElute 2, and the Elute series of HPLCs. The nanoElute 2 uses UHPLC technology focused on 4-D proteomics. Key specifications: flow rate range (50 to 2000 nL/min); gradient delay (<0.4 uL); Pmax: 1000 bar.
All three of the Elute Series of HPLCs have a flow rate range of 1 to 5,000 uL/min. All have Pmax of 1,300 bar. The UHPLC model is designed for fast, high-resolution separations. The Elute OLE combines UHPLC with online liquid extraction. The Elute HT combines a PAL3 autosampler for high throughput applications.
Mass spectrometry
Plasmion GMBH introduced a novel compact soft ionization source, SICRIT, that fits on the cone of most any mass spectrometers for direct detection, specimen imaging or chromatography-MS. Their product name is an acronym for “Soft Ionization by Chemical Reaction in Transfer.” The patented ion source extends the MS inlet and ionizes the molecules with a cold plasma produced by a dielectric barrier discharge (DBD). The unique shape of the plasma is designed to avoid fragmentation of analyte ions. The design is compatible with all current LC-MS, GC-MS and SFC instruments. However, with direct MS analysis, one can avoid the separation stage entirely.
Shimadzu introduced seven new instruments including five new mass spectrometers at Pittcon. Their LCMS-9050 Quadrupole Time-of-Flight (Q-TOF) LC-MS incorporates prior advances to provide long-term mass accuracy provided by high precision temperature control. The resolving power specification is an industry-leading 45,000. Shimadzu’s patent-pending UFstabilization algorithm provides fast polarity switching and stabilization. Options include the NEXERA UC Supercritical Fluid Extraction/Chromatograph System and NEXERA Mikros Micro Flowrate Range LC-MS for narrow bore and capillary column technology, which provides comprehensive assay of trace components. Shimadzu boasts that the LCMS-9050 system qualifies as an eco-friendly instrument since it reduces mobile phase solvent consumption by 25%.
Spectrophotometers
Mettler Toledo introduced the EasyPlus line of spectrophotometers, which differ only in their lamp wavelength range. The Easy VIS uses a tungsten lamp for photometry in the range 330 to 1000 nm. A xenon flash lamp in the Easy UV extends the range to 190 nm. Operation is simple: Record the blank then select and record the sample. The software does the rest. For colorimetry, the Easy uses spectral ranges specified by ICUMSA for sugar color, ESBC for beer quality analysis, or OIV CIELab for wine color determination.
Shimadzu’s AA-7800 Series Atomic Absorption spectrometers are an update over prior series. The instruments are compact, requiring less than a meter of bench space. Double beam optics and atomizer improve data acquisition. Shimadzu’s WizAArd software facilitates setting instrument parameters and validation per requirements of FDA 21 CFR part 11.
Mergers and acquisitions
Waters Associates started selling Styragel columns for steric exclusion chromatography in the mid-1960s. Instruments came a few years later. A decade later, Wyatt Technologies jumped in with light scattering instruments, which were useful for polymers, particularly polystyrene. Over the decades, Waters and Wyatt both had booths in Pittcon’s exhibition in close proximity, sometimes across the aisle. Fast forward to December 2022, and they merged. Wyatt will become an operating company and brand under the Waters Corporation, much as Andrew Alliance and TA Instruments. Mergers often flounder as corporate cultures clash. However, both Waters and Wyatt have very similar customer-centric commercial philosophies. I do not expect culture clash to be a problem. Some may recall when Millipore acquired Waters, where the culture clash was spectacular. A few years later, Millipore divested.
Recently, Bruker acquired IonSense to “accelerate DART-MS methods and applications.” The DART ion source is very popular in labs that appreciate the ability to analyze semi volatiles directly and in real-time. At Pittcon 23, the DART was mounted on the Bruker EVOC MS. The combination was the most popular MS product in the Bruker booth, according to representatives. Interestingly, PFAS analysis is the top application.
Looking forward to Pittcon 2024
Next year, Pittcon will cross the Rockies for the first ever meeting on the West Coast—San Diego from February 24 to 28, 2024. The San Diego region is home to many scientific startups, especially in biotechnology and modern photonics. I expect major advances in photonics, including sculptured light, applied artificial intelligence and nanomaterials. See you there!
About the Author: Robert Stevenson, Ph.D., is a member of Labcompare's Editorial Advisory Board and Editor Emeritus of Labcompare and American Laboratory. He has been involved in developing instrumentation and enabled applications since the late 1960's at firms including Varian, Altex, Bio-Rad, and TosoHaas. Stevenson has been a regular contributor to American Laboratory since its founding in 1968. He has authored more than 450 papers on new technology and applications.